+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1061 started at 14:10:48 on 06-Sep-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1061 in P-1 CELL 0.71073 6.7104 9.9705 12.0246 106.093 90.916 90.823 ZERR 1.00 0.0001 0.0003 0.0004 0.001 0.002 0.002 LATT 1 SFAC C H O FE BR IN UNIT 28 20 8 4 2 2 V = 772.74 F(000) = 524.0 Mu = 5.93 mm-1 Cell Wt = 1097.30 Rho = 2.358 MERG 2 OMIT -3.00 55.00 OMIT 1 0 0 OMIT 0 1 1 FMAP 2 PLAN 25 SIZE 0.02 0.10 0.10 ACTA WGHT 0.01840 0.79580 L.S. 5 TEMP -153.00 FVAR 0.52818 C1 1 0.218456 0.395818 0.101504 11.00000 0.01801 0.01828 = 0.01440 0.00677 -0.00088 -0.00441 C2 1 -0.136098 0.492071 0.142518 11.00000 0.02203 0.01953 = 0.01465 0.00701 0.00295 0.00328 C3 1 0.179968 0.696148 0.349374 11.00000 0.03513 0.01308 = 0.01371 0.00091 -0.00011 -0.00538 AFIX 43 H3 2 0.160287 0.689965 0.425874 11.00000 -1.20000 AFIX 0 C4 1 0.041416 0.746737 0.281348 11.00000 0.02795 0.00991 = 0.03046 0.00012 0.00342 0.00192 AFIX 43 H4 2 -0.088381 0.779170 0.303630 11.00000 -1.20000 AFIX 0 C5 1 0.131775 0.740283 0.173140 11.00000 0.03564 0.01453 = 0.02356 0.00912 -0.00696 -0.00331 AFIX 43 H5 2 0.072933 0.768881 0.111251 11.00000 -1.20000 AFIX 0 C6 1 0.321520 0.684667 0.174115 11.00000 0.02717 0.01660 = 0.01819 0.00366 0.00299 -0.00882 AFIX 43 H6 2 0.413807 0.668386 0.112923 11.00000 -1.20000 AFIX 0 C7 1 0.352464 0.656529 0.283475 11.00000 0.02187 0.01719 = 0.01963 0.00341 -0.00615 -0.00572 AFIX 43 H7 2 0.468683 0.617961 0.307496 11.00000 -1.20000 AFIX 0 C8 1 0.054637 0.084803 0.169739 11.00000 0.01932 0.01128 = 0.01844 0.00396 -0.00367 -0.00279 C9 1 0.035194 0.106677 0.384013 11.00000 0.02266 0.01023 = 0.01775 0.00169 0.00589 -0.00091 C10 1 -0.353110 -0.004549 0.189209 11.00000 0.01859 0.02105 = 0.03864 -0.01043 -0.00024 -0.00483 AFIX 43 H10 2 -0.330428 -0.093192 0.136490 11.00000 -1.20000 AFIX 0 C11 1 -0.368498 0.123950 0.160505 11.00000 0.01540 0.03739 = 0.01951 -0.00130 -0.00436 -0.00253 AFIX 43 H11 2 -0.357055 0.136198 0.085267 11.00000 -1.20000 AFIX 0 C12 1 -0.403624 0.229960 0.262793 11.00000 0.01505 0.01895 = 0.02757 0.00366 -0.00258 0.00071 AFIX 43 H12 2 -0.421860 0.325948 0.268576 11.00000 -1.20000 AFIX 0 C13 1 -0.406965 0.168168 0.355579 11.00000 0.01649 0.02372 = 0.02291 0.00026 0.00508 -0.00100 AFIX 43 H13 2 -0.425673 0.215372 0.434841 11.00000 -1.20000 AFIX 0 C14 1 -0.377147 0.022241 0.308401 11.00000 0.01767 0.02071 = 0.04635 0.01123 0.00708 -0.00329 AFIX 43 H14 2 -0.374155 -0.045175 0.350818 11.00000 -1.20000 AFIX 0 O1 3 0.293166 0.304781 0.034944 11.00000 0.02948 0.01835 = 0.02057 0.00103 0.00809 0.00414 O2 3 -0.297025 0.462789 0.107884 11.00000 0.02006 0.04281 = 0.02274 0.01243 -0.00294 -0.00240 O3 3 0.168819 0.044839 0.098143 11.00000 0.02470 0.02490 = 0.02046 0.00038 0.00829 -0.00052 O4 3 0.143941 0.082702 0.450573 11.00000 0.02942 0.02289 = 0.02304 0.01013 -0.00229 -0.00045 FE1 4 0.106528 0.539361 0.196542 11.00000 0.01558 0.01139 = 0.01030 0.00197 0.00062 0.00016 FE2 4 -0.127032 0.134714 0.276165 11.00000 0.01442 0.01120 = 0.01384 0.00048 0.00160 -0.00062 BR1 5 -0.250816 0.557802 0.477793 11.00000 0.01353 0.01634 = 0.01270 0.00082 -0.00048 0.00203 IN1 6 0.014774 0.383293 0.324884 11.00000 0.01533 0.01045 = 0.01003 0.00180 0.00043 -0.00064 HKLF 4 Covalent radii and connectivity table for 2005src1061 in P-1 C 0.770 H 0.320 O 0.660 FE 1.240 BR 1.140 IN 1.440 C1 - O1 Fe1 C2 - O2 Fe1 C3 - C7 C4 Fe1 C4 - C3 C5 Fe1 C5 - C6 C4 Fe1 C6 - C5 C7 Fe1 C7 - C3 C6 Fe1 C8 - O3 Fe2 C9 - O4 Fe2 C10 - C14 C11 Fe2 C11 - C12 C10 Fe2 C12 - C11 C13 Fe2 C13 - C12 C14 Fe2 C14 - C10 C13 Fe2 O1 - C1 O2 - C2 O3 - C8 O4 - C9 Fe1 - C2 C1 C4 C7 C3 C6 C5 In1 Fe2 - C8 C9 C10 C11 C14 C13 C12 In1 Br1 - In1_$1 In1 In1 - Fe2 Fe1 Br1_$1 Br1 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 18318 Reflections read, of which 5 rejected -8 =< h =< 8, -12 =< k =< 12, -15 =< l =< 15, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 3538 Unique reflections, of which 0 suppressed R(int) = 0.0350 R(sigma) = 0.0280 Friedel opposites merged Maximum memory for data reduction = 1935 / 34876 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2452 / 248715 wR2 = 0.0512 before cycle 1 for 3538 data and 199 / 199 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52782 0.00048 -0.748 OSF Mean shift/esd = 0.062 Maximum = -0.748 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2452 / 248715 wR2 = 0.0512 before cycle 2 for 3538 data and 199 / 199 parameters GooF = S = 1.109; Restrained GooF = 1.109 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52768 0.00048 -0.290 OSF Mean shift/esd = 0.020 Maximum = -0.290 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2452 / 248715 wR2 = 0.0513 before cycle 3 for 3538 data and 199 / 199 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52768 0.00048 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for y C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2452 / 248715 wR2 = 0.0513 before cycle 4 for 3538 data and 199 / 199 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52768 0.00048 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z In1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2452 / 248715 wR2 = 0.0513 before cycle 5 for 3538 data and 199 / 199 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52768 0.00048 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z In1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O2 Largest correlation matrix elements 0.509 U22 In1 / OSF 0.503 U33 In1 / OSF Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.1602 0.6900 0.4259 43 0.950 0.000 C3 C7 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 -0.0884 0.7791 0.3036 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.0729 0.7689 0.1113 43 0.950 0.000 C5 C6 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.4138 0.6684 0.1129 43 0.950 0.000 C6 C5 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.4687 0.6179 0.3075 43 0.950 0.000 C7 C3 C6 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C10 ** H10 -0.3306 -0.0932 0.1364 43 0.950 0.000 C10 C14 C11 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C11 ** H11 -0.3570 0.1362 0.0853 43 0.950 0.000 C11 C12 C10 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C12 ** H12 -0.4219 0.3260 0.2686 43 0.950 0.000 C12 C11 C13 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C13 ** H13 -0.4257 0.2154 0.4348 43 0.950 0.000 C13 C12 C14 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C14 ** H14 -0.3741 -0.0452 0.3508 43 0.950 0.000 C14 C10 C13 2005src1061 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21847 0.39583 0.10150 1.00000 0.01792 0.01814 0.01434 0.00673 -0.00092 -0.00442 0.01642 0.00490 0.00039 0.00027 0.00022 0.00000 0.00131 0.00130 0.00124 0.00104 0.00101 0.00100 0.00052 C2 -0.13606 0.49204 0.14252 1.00000 0.02201 0.01935 0.01460 0.00697 0.00300 0.00332 0.01815 0.00527 0.00041 0.00028 0.00022 0.00000 0.00146 0.00133 0.00127 0.00104 0.00105 0.00103 0.00054 C3 0.17994 0.69617 0.34937 1.00000 0.03491 0.01296 0.01364 0.00084 -0.00011 -0.00532 0.02114 0.00504 0.00044 0.00027 0.00023 0.00000 0.00163 0.00127 0.00127 0.00100 0.00111 0.00107 0.00058 H3 0.16025 0.69001 0.42588 1.00000 0.02537 0.00000 0.00000 C4 0.04142 0.74673 0.28134 1.00000 0.02791 0.00984 0.03022 0.00004 0.00340 0.00206 0.02371 0.00533 0.00045 0.00027 0.00025 0.00000 0.00157 0.00127 0.00157 0.00111 0.00122 0.00105 0.00061 H4 -0.08839 0.77914 0.30362 1.00000 0.02845 0.00000 0.00000 C5 0.13178 0.74029 0.17314 1.00000 0.03547 0.01442 0.02346 0.00915 -0.00696 -0.00333 0.02379 0.00535 0.00045 0.00028 0.00025 0.00000 0.00169 0.00132 0.00146 0.00111 0.00122 0.00112 0.00061 H5 0.07294 0.76890 0.11125 1.00000 0.02855 0.00000 0.00000 C6 0.32151 0.68468 0.17412 1.00000 0.02712 0.01651 0.01799 0.00359 0.00301 -0.00882 0.02084 0.00501 0.00042 0.00027 0.00023 0.00000 0.00151 0.00132 0.00134 0.00105 0.00110 0.00106 0.00057 H6 0.41381 0.66841 0.11293 1.00000 0.02501 0.00000 0.00000 C7 0.35246 0.65652 0.28348 1.00000 0.02179 0.01717 0.01955 0.00343 -0.00617 -0.00577 0.01997 0.00489 0.00041 0.00027 0.00023 0.00000 0.00141 0.00133 0.00136 0.00106 0.00108 0.00102 0.00056 H7 0.46866 0.61793 0.30751 1.00000 0.02396 0.00000 0.00000 C8 0.05466 0.08480 0.16975 1.00000 0.01932 0.01128 0.01825 0.00394 -0.00364 -0.00279 0.01639 0.00475 0.00039 0.00025 0.00022 0.00000 0.00135 0.00120 0.00131 0.00100 0.00107 0.00097 0.00053 C9 0.03516 0.10668 0.38400 1.00000 0.02251 0.01023 0.01767 0.00170 0.00587 -0.00087 0.01719 0.00501 0.00040 0.00025 0.00023 0.00000 0.00140 0.00121 0.00131 0.00100 0.00109 0.00098 0.00054 C10 -0.35316 -0.00456 0.18918 1.00000 0.01853 0.02088 0.03842 -0.01043 -0.00021 -0.00482 0.02974 0.00541 0.00043 0.00031 0.00028 0.00000 0.00148 0.00149 0.00178 0.00127 0.00125 0.00110 0.00070 H10 -0.33056 -0.09321 0.13644 1.00000 0.03569 0.00000 0.00000 C11 -0.36848 0.12396 0.16050 1.00000 0.01535 0.03729 0.01943 -0.00136 -0.00428 -0.00251 0.02595 0.00529 0.00041 0.00032 0.00025 0.00000 0.00139 0.00173 0.00142 0.00123 0.00109 0.00116 0.00064 H11 -0.35698 0.13621 0.08527 1.00000 0.03114 0.00000 0.00000 C12 -0.40363 0.22998 0.26279 1.00000 0.01501 0.01873 0.02748 0.00363 -0.00255 0.00079 0.02099 0.00518 0.00039 0.00028 0.00025 0.00000 0.00133 0.00136 0.00150 0.00113 0.00109 0.00101 0.00057 H12 -0.42186 0.32597 0.26857 1.00000 0.02519 0.00000 0.00000 C13 -0.40698 0.16817 0.35557 1.00000 0.01645 0.02363 0.02273 0.00024 0.00509 -0.00099 0.02213 0.00535 0.00040 0.00029 0.00025 0.00000 0.00136 0.00144 0.00142 0.00113 0.00108 0.00106 0.00058 H13 -0.42571 0.21538 0.43482 1.00000 0.02656 0.00000 0.00000 C14 -0.37714 0.02223 0.30841 1.00000 0.01759 0.02067 0.04626 0.01127 0.00709 -0.00329 0.02774 0.00592 0.00042 0.00030 0.00029 0.00000 0.00144 0.00146 0.00191 0.00133 0.00127 0.00108 0.00066 H14 -0.37410 -0.04518 0.35084 1.00000 0.03329 0.00000 0.00000 O1 0.29315 0.30475 0.03493 1.00000 0.02939 0.01831 0.02051 0.00103 0.00812 0.00416 0.02349 0.00382 0.00030 0.00020 0.00017 0.00000 0.00112 0.00099 0.00101 0.00081 0.00083 0.00080 0.00042 O2 -0.29702 0.46279 0.10787 1.00000 0.01993 0.04265 0.02270 0.01246 -0.00299 -0.00247 0.02782 0.00398 0.00030 0.00023 0.00017 0.00000 0.00110 0.00129 0.00106 0.00093 0.00084 0.00088 0.00046 O3 0.16880 0.04485 0.09814 1.00000 0.02467 0.02469 0.02047 0.00036 0.00830 -0.00050 0.02438 0.00380 0.00030 0.00020 0.00017 0.00000 0.00106 0.00106 0.00102 0.00082 0.00083 0.00080 0.00043 O4 0.14395 0.08270 0.45057 1.00000 0.02937 0.02276 0.02300 0.01013 -0.00234 -0.00045 0.02433 0.00384 0.00030 0.00020 0.00017 0.00000 0.00113 0.00104 0.00104 0.00084 0.00087 0.00082 0.00043 Fe1 0.10653 0.53936 0.19654 1.00000 0.01550 0.01130 0.01023 0.00196 0.00062 0.00017 0.01255 0.00066 0.00005 0.00004 0.00003 0.00000 0.00019 0.00018 0.00017 0.00013 0.00014 0.00013 0.00009 Fe2 -0.12703 0.13471 0.27617 1.00000 0.01435 0.01112 0.01376 0.00046 0.00160 -0.00062 0.01367 0.00067 0.00005 0.00004 0.00003 0.00000 0.00019 0.00018 0.00018 0.00014 0.00014 0.00013 0.00009 Br1 -0.25082 0.55780 0.47779 1.00000 0.01345 0.01627 0.01263 0.00080 -0.00048 0.00203 0.01475 0.00045 0.00004 0.00002 0.00002 0.00000 0.00013 0.00013 0.00013 0.00010 0.00009 0.00009 0.00007 In1 0.01478 0.38329 0.32488 1.00000 0.01525 0.01037 0.00997 0.00178 0.00043 -0.00064 0.01208 0.00031 0.00002 0.00002 0.00001 0.00000 0.00010 0.00010 0.00009 0.00007 0.00007 0.00006 0.00006 Final Structure Factor Calculation for 2005src1061 in P-1 Total number of l.s. parameters = 199 Maximum vector length = 511 Memory required = 2253 / 25039 wR2 = 0.0513 before cycle 6 for 3538 data and 0 / 199 parameters GooF = S = 1.110; Restrained GooF = 1.110 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0184 * P )^2 + 0.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0230 for 3276 Fo > 4sig(Fo) and 0.0261 for all 3538 data wR2 = 0.0513, GooF = S = 1.110, Restrained GooF = 1.110 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0231 0.0144 0.0118 C1 0.0243 0.0174 0.0127 C2 0.0366 0.0165 0.0104 C3 0.0346 0.0273 0.0093 C4 0.0396 0.0203 0.0114 C5 0.0343 0.0174 0.0108 C6 0.0281 0.0206 0.0112 C7 0.0230 0.0159 0.0103 C8 0.0271 0.0144 0.0101 C9 0.0576 0.0208 0.0108 C10 0.0448 0.0215 0.0115 C11 0.0301 0.0185 0.0143 C12 0.0332 0.0194 0.0138 C13 0.0478 0.0232 0.0122 C14 0.0337 0.0240 0.0127 O1 0.0432 0.0228 0.0175 O2 0.0356 0.0237 0.0138 O3 0.0309 0.0247 0.0174 O4 0.0155 0.0123 0.0098 Fe1 0.0178 0.0134 0.0098 Fe2 0.0201 0.0127 0.0114 Br1 0.0155 0.0114 0.0093 In1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.057 0.085 0.113 0.148 0.183 0.226 0.282 0.371 1.000 Number in group 359. 352. 358. 345. 362. 349. 351. 356. 356. 350. GooF 1.022 1.154 1.210 1.205 1.173 1.017 0.902 0.930 1.078 1.327 K 1.206 0.951 0.938 0.956 0.963 0.985 1.000 1.009 1.019 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 364. 351. 346. 363. 344. 364. 349. 353. 354. 350. GooF 1.263 1.070 1.086 1.050 0.983 0.997 1.025 0.985 1.090 1.452 K 0.959 0.990 1.009 1.007 1.021 1.019 1.028 1.020 1.007 0.971 R1 0.059 0.044 0.038 0.031 0.025 0.022 0.019 0.015 0.015 0.019 Recommended weighting scheme: WGHT 0.0174 0.8206 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 7 7 0 166.26 269.22 4.17 0.085 0.78 0 3 0 458.77 356.78 4.00 0.098 3.19 -1 1 2 32863.79 36908.66 3.93 1.000 3.74 -5 4 2 38.03 1.94 3.76 0.007 1.13 -1 1 0 9913.70 11026.08 3.55 0.547 5.55 3 2 9 341.43 500.38 3.43 0.116 1.02 2 3 0 1055.59 1196.51 3.21 0.180 2.29 3 -3 4 1415.65 1590.65 3.21 0.208 1.67 2 -3 3 1364.62 1541.36 3.18 0.204 2.19 -2 0 3 21996.01 24269.09 3.13 0.811 2.56 -4 10 3 36.87 98.09 3.13 0.052 0.78 -4 -11 4 653.26 806.63 3.06 0.148 0.79 -1 2 13 88.35 164.80 3.03 0.067 0.83 0 -11 7 -0.34 33.81 3.02 0.030 0.88 2 -4 5 133.01 97.29 3.00 0.051 1.69 2 -7 13 171.37 253.91 2.98 0.083 0.83 1 -1 1 10502.59 11515.61 2.92 0.559 5.31 -1 7 8 236.60 319.08 2.92 0.093 0.87 -1 6 0 131.06 96.31 2.91 0.051 1.56 -1 -1 5 202.98 159.57 2.89 0.066 2.27 0 0 2 11890.88 13017.21 2.87 0.594 5.78 3 1 0 24.81 11.66 2.84 0.018 2.17 0 -2 1 760.16 663.05 2.84 0.134 4.93 -5 -2 11 2615.54 2203.32 2.82 0.244 0.85 -6 6 1 604.79 711.02 2.81 0.139 0.91 -5 7 2 193.06 263.12 2.78 0.084 0.93 -2 -9 13 503.77 631.53 2.77 0.131 0.78 2 9 7 55.41 122.97 2.77 0.058 0.77 1 7 9 165.88 236.29 2.76 0.080 0.82 8 4 0 301.82 488.10 2.75 0.115 0.79 3 9 2 154.81 210.89 2.75 0.076 0.90 -1 -3 1 26635.78 28675.38 2.72 0.881 2.96 -3 0 2 521.27 434.56 2.70 0.109 2.10 -3 2 1 7526.80 8132.41 2.69 0.469 1.98 3 -11 9 174.36 267.09 2.69 0.085 0.78 -1 -3 2 15364.57 16524.68 2.67 0.669 2.88 -5 -3 7 6559.11 6036.07 2.66 0.404 1.05 5 1 0 3600.96 3249.88 2.65 0.297 1.33 2 0 2 21905.15 23455.98 2.64 0.797 2.87 7 -5 3 729.74 845.02 2.64 0.151 0.86 4 1 1 7151.46 7686.82 2.64 0.456 1.61 3 -2 3 1384.59 1256.19 2.63 0.184 1.88 -8 -2 5 274.11 384.13 2.62 0.102 0.79 -1 1 7 76.86 49.59 2.62 0.037 1.52 -1 -6 11 82.86 122.04 2.60 0.058 1.01 -2 -2 1 171.33 137.02 2.59 0.061 2.76 -1 1 4 2321.70 2538.18 2.58 0.262 2.42 3 -5 5 222.99 272.21 2.58 0.086 1.37 -1 -9 7 131.38 177.15 2.57 0.069 1.02 0 5 3 315.36 262.39 2.53 0.084 1.55 Bond lengths and angles C1 - Distance Angles O1 1.1573 (0.0033) Fe1 1.7521 (0.0027) 176.71 (0.23) C1 - O1 C2 - Distance Angles O2 1.1552 (0.0033) Fe1 1.7518 (0.0028) 178.96 (0.26) C2 - O2 C3 - Distance Angles C7 1.4118 (0.0041) C4 1.4160 (0.0041) 107.96 (0.24) Fe1 2.1025 (0.0026) 70.11 (0.15) 69.88 (0.15) C3 - C7 C4 C4 - Distance Angles C3 1.4160 (0.0041) C5 1.4300 (0.0042) 107.80 (0.26) Fe1 2.0921 (0.0026) 70.67 (0.15) 70.51 (0.15) C4 - C3 C5 C5 - Distance Angles C6 1.3972 (0.0042) C4 1.4300 (0.0042) 108.23 (0.25) Fe1 2.1038 (0.0026) 70.57 (0.15) 69.63 (0.15) C5 - C6 C4 C6 - Distance Angles C5 1.3972 (0.0042) C7 1.4315 (0.0038) 108.02 (0.25) Fe1 2.1029 (0.0026) 70.63 (0.15) 69.81 (0.14) C6 - C5 C7 C7 - Distance Angles C3 1.4118 (0.0041) C6 1.4315 (0.0038) 107.98 (0.24) Fe1 2.0961 (0.0025) 70.60 (0.15) 70.33 (0.14) C7 - C3 C6 C8 - Distance Angles O3 1.1516 (0.0032) Fe2 1.7567 (0.0027) 176.20 (0.22) C8 - O3 C9 - Distance Angles O4 1.1504 (0.0032) Fe2 1.7631 (0.0028) 176.73 (0.23) C9 - O4 C10 - Distance Angles C14 1.3961 (0.0046) C11 1.4210 (0.0045) 108.05 (0.25) Fe2 2.0996 (0.0027) 70.83 (0.16) 70.25 (0.15) C10 - C14 C11 C11 - Distance Angles C12 1.4077 (0.0039) C10 1.4210 (0.0045) 108.22 (0.26) Fe2 2.1003 (0.0028) 71.32 (0.16) 70.20 (0.16) C11 - C12 C10 C12 - Distance Angles C11 1.4077 (0.0039) C13 1.4165 (0.0041) 107.88 (0.25) Fe2 2.1210 (0.0027) 69.73 (0.16) 70.00 (0.15) C12 - C11 C13 C13 - Distance Angles C12 1.4165 (0.0041) C14 1.4260 (0.0040) 107.59 (0.25) Fe2 2.1096 (0.0027) 70.87 (0.16) 70.07 (0.16) C13 - C12 C14 C14 - Distance Angles C10 1.3961 (0.0046) C13 1.4260 (0.0040) 108.26 (0.27) Fe2 2.1054 (0.0028) 70.39 (0.16) 70.39 (0.15) C14 - C10 C13 O1 - Distance Angles C1 1.1573 (0.0033) O1 - O2 - Distance Angles C2 1.1552 (0.0033) O2 - O3 - Distance Angles C8 1.1516 (0.0032) O3 - O4 - Distance Angles C9 1.1504 (0.0032) O4 - Fe1 - Distance Angles C2 1.7518 (0.0028) C1 1.7521 (0.0027) 94.91 (0.12) C4 2.0921 (0.0026) 95.54 (0.12) 159.99 (0.12) C7 2.0961 (0.0026) 161.73 (0.12) 102.63 (0.12) 66.20 (0.11) C3 2.1025 (0.0026) 125.12 (0.12) 138.60 (0.12) 39.46 (0.11) 39.30 (0.11) C6 2.1029 (0.0026) 134.45 (0.11) 94.45 (0.11) 66.19 (0.11) 39.86 (0.10) 66.31 (0.11) C5 2.1038 (0.0026) 100.50 (0.12) 121.15 (0.12) 39.85 (0.12) 66.04 (0.11) 66.28 (0.11) 38.80 (0.11) In1 2.5527 (0.0004) 81.66 (0.08) 88.79 (0.08) 109.58 (0.08) 103.54 (0.08) 87.28 (0.07) 143.02 (0.08) 149.35 (0.08) Fe1 - C2 C1 C4 C7 C3 C6 C5 Fe2 - Distance Angles C8 1.7567 (0.0027) C9 1.7631 (0.0028) 91.92 (0.12) C10 2.0996 (0.0027) 97.08 (0.12) 125.25 (0.12) C11 2.1003 (0.0028) 96.03 (0.12) 163.64 (0.12) 39.55 (0.12) C14 2.1054 (0.0028) 129.71 (0.12) 98.34 (0.12) 38.78 (0.13) 65.65 (0.12) C13 2.1096 (0.0027) 161.02 (0.11) 104.58 (0.12) 65.82 (0.11) 65.68 (0.11) 39.55 (0.11) C12 2.1210 (0.0027) 127.72 (0.12) 139.16 (0.11) 65.77 (0.11) 38.96 (0.11) 65.73 (0.11) 39.12 (0.11) In1 2.5497 (0.0004) 88.61 (0.08) 87.55 (0.08) 146.25 (0.09) 106.87 (0.09) 140.61 (0.08) 101.22 (0.08) 84.45 (0.07) Fe2 - C8 C9 C10 C11 C14 C13 C12 Br1 - Distance Angles In1_$1 2.7503 (0.0003) In1 2.8293 (0.0003) 98.23 (0.01) Br1 - In1_$1 In1 - Distance Angles Fe2 2.5497 (0.0004) Fe1 2.5527 (0.0004) 131.59 (0.01) Br1_$1 2.7503 (0.0003) 110.99 (0.01) 111.47 (0.01) Br1 2.8293 (0.0003) 107.56 (0.01) 100.48 (0.01) 81.77 (0.01) In1 - Fe2 Fe1 Br1_$1 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0253 for 3538 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.63 at 0.3373 0.6016 0.4003 [ 1.47 A from H3 ] Deepest hole -0.74 at 0.0526 0.5632 0.6982 [ 0.81 A from IN1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 2351 / 20037 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3373 0.6016 0.4003 1.00000 0.05 0.63 1.47 H3 1.48 H7 1.65 C3 1.65 C7 Q2 1 0.2801 0.2083 0.1742 1.00000 0.05 0.62 1.78 O3 1.93 C8 2.15 O1 2.31 C1 Q3 1 -0.2176 0.3163 0.1226 1.00000 0.05 0.61 1.62 O2 1.78 C2 1.95 H11 2.23 H12 Q4 1 -0.1304 0.4850 -0.0095 1.00000 0.05 0.58 1.81 C2 1.87 O2 1.93 C1 2.20 FE1 Q5 1 -0.3754 0.0748 0.0747 1.00000 0.05 0.52 0.60 H11 1.01 C11 1.77 C10 2.04 H10 Q6 1 0.0079 0.2265 0.2993 1.00000 0.05 0.50 1.25 FE2 1.51 IN1 1.78 C9 1.82 C8 Q7 1 -0.1710 0.7171 0.3533 1.00000 0.05 0.47 1.12 H4 1.74 C4 2.37 C3 2.42 H3 Q8 1 0.3766 0.3618 0.0422 1.00000 0.05 0.46 0.78 O1 1.28 C1 2.31 H6 2.42 O2 Q9 1 -0.3875 0.3177 0.4308 1.00000 0.05 0.44 1.06 H13 1.52 C13 1.97 C12 1.99 H12 Q10 1 0.0132 0.1971 0.3763 1.00000 0.05 0.42 0.94 C9 1.50 FE2 1.85 O4 2.11 IN1 Q11 1 -0.0061 -0.0680 0.2053 1.00000 0.05 0.40 1.74 C8 1.80 H5 2.08 C5 2.14 FE2 Q12 1 0.1204 0.4201 0.2376 1.00000 0.05 0.39 1.40 IN1 1.41 FE1 1.73 C1 2.28 C2 Q13 1 0.0231 0.8815 0.2710 1.00000 0.05 0.38 1.39 C4 1.40 H4 1.74 C5 1.97 H5 Q14 1 -0.1404 0.4294 0.2616 1.00000 0.05 0.37 1.43 IN1 1.71 C2 2.15 H12 2.22 O2 Q15 1 -0.0515 0.5382 0.2170 1.00000 0.05 0.37 1.04 C2 1.09 FE1 2.09 O2 2.09 C4 Q16 1 0.1049 0.1864 0.4798 1.00000 0.05 0.37 1.03 O4 1.28 C9 2.31 H3 2.53 H4 Q17 1 0.1321 0.2053 0.2382 1.00000 0.05 0.36 1.35 C8 1.97 FE2 1.97 IN1 2.00 O3 Q18 1 -0.0618 0.2285 0.4584 1.00000 0.05 0.36 1.46 C9 1.57 H3 2.00 O4 2.17 FE2 Q19 1 0.0035 0.4792 0.2620 1.00000 0.05 0.36 1.31 FE1 1.38 IN1 1.74 C2 2.39 C1 Q20 1 -0.1099 0.1605 0.0185 1.00000 0.05 0.36 1.90 H11 1.90 H5 2.16 O3 2.41 C8 Q21 1 0.1520 0.3012 0.3613 1.00000 0.05 0.35 1.38 IN1 2.14 BR1 2.17 C9 2.49 FE2 Q22 1 -0.3472 0.1134 0.3423 1.00000 0.05 0.35 0.67 C13 0.90 C14 1.40 H13 1.62 H14 Q23 1 0.1148 -0.0418 0.5189 1.00000 0.05 0.35 1.68 O4 1.80 C9 1.84 O4 2.31 H14 Q24 1 -0.0347 0.2864 0.1421 1.00000 0.05 0.35 2.14 C1 2.16 IN1 2.17 C2 2.22 C8 Q25 1 0.2833 0.1669 0.3764 1.00000 0.05 0.35 1.67 O4 1.77 C9 2.07 H13 2.10 C13 Shortest distances between peaks (including symmetry equivalents) 15 19 0.97 12 19 0.99 6 10 1.05 11 13 1.06 14 19 1.08 10 18 1.08 6 17 1.10 16 18 1.25 2 17 1.27 3 24 1.30 6 21 1.30 10 16 1.41 10 21 1.43 14 15 1.46 17 21 1.53 21 25 1.66 16 25 1.71 20 24 1.72 12 15 1.72 4 4 1.77 12 14 1.78 3 14 1.80 12 24 1.80 10 25 1.84 3 20 1.87 23 23 1.87 10 17 1.88 14 24 1.88 17 24 1.93 6 18 1.97 18 23 1.98 1 9 1.99 7 16 2.01 9 22 2.04 16 23 2.05 17 25 2.06 19 24 2.07 16 21 2.09 18 21 2.11 12 17 2.15 6 24 2.15 12 21 2.15 5 20 2.16 6 25 2.22 7 15 2.23 2 12 2.32 2 24 2.32 2 6 2.36 2 21 2.36 4 8 2.37 6 12 2.37 6 16 2.40 10 23 2.41 6 14 2.42 9 18 2.42 15 24 2.43 18 22 2.43 3 15 2.43 3 19 2.45 16 23 2.45 7 13 2.50 22 23 2.52 3 5 2.53 10 22 2.54 18 25 2.55 22 25 2.56 5 5 2.57 2 8 2.58 2 25 2.58 19 21 2.60 7 19 2.62 9 25 2.62 7 18 2.65 1 12 2.66 4 15 2.67 3 12 2.68 3 4 2.68 6 19 2.68 11 20 2.72 6 22 2.74 4 15 2.75 13 23 2.77 7 14 2.79 11 17 2.79 14 21 2.79 1 18 2.79 2 5 2.80 17 19 2.82 1 19 2.82 6 11 2.84 14 17 2.86 10 11 2.86 21 24 2.87 8 12 2.87 13 23 2.92 17 18 2.92 3 6 2.93 3 8 2.96 9 10 2.97 16 17 2.97 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.01: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.93: Structure factors and derivatives 1.61: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.07: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1061 finished at 14:10:52 Total CPU time: 4.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++